CN105236473B - Method for preparing shell-structured stannous oxide material - Google Patents
Method for preparing shell-structured stannous oxide material Download PDFInfo
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- CN105236473B CN105236473B CN201510717867.3A CN201510717867A CN105236473B CN 105236473 B CN105236473 B CN 105236473B CN 201510717867 A CN201510717867 A CN 201510717867A CN 105236473 B CN105236473 B CN 105236473B
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- tin monoxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a method for preparing a shell-structured stannous oxide material. According to the method, SnCl2.2H2O serves as a tin source, citric acid and the like serve as a reducer, shell-structured stannous oxide powder with the grain size of 10-20 microns is prepared by adopting a one-step hydrothermal method, and shell-structured stannous oxide consists of flakes with the thickness of 1-2 microns. The structure is special, so that the shell-structured stannous oxide material is expected to have a good application in aspects of lithium-/sodium-ion battery cathode materials, chemical synthesis catalysts and the like. The method is short in preparation cycle, simple in process, high in repeatability, low in reaction temperature, low in energy consumption and reduced in production cost, thereby being applicable to large-scale production preparation.
Description
Technical field
The present invention relates to the preparation of a kind of Tin monoxide material, be specifically related to a kind of shelly texture Tin monoxide powder body
Preparation method.
Background technology
At present, carbon based negative electrodes material and titanio negative material are respectively provided with preferable cyclical stability, but capacity is only
200～300mAh g-1.And due to its limited avtive spot, capacity is difficult to improve a lot.Therefore, exploitation
The novel negative material with high power capacity is highly significant.In the research of anticathode material, find SnO2Storage sodium hold
Amount is 667mAh g-1, it is far longer than graphite and the theoretical capacity of titanio negative material, causes the wide of battery material circle
General concern.Nearest research finds, for stannum oxide negative material, Tin monoxide negative material follows including
Ring performance shows the most excellent (Electrochemical properties of tin oxide in terms of interior chemical property
anodes for sodium-ion batteries.Journal of Power Sources.2015；284:287-295), because aoxidizing
The hypopolarization of stannous makes it have preferable electric conductivity, and this is conducive to the quick transmission of electronics.
But, similar to alloy type simple substance, Tin monoxide negative material has the biggest bulk effect, causes in charge and discharge
The powder of detached of material in electric process, reduces efficiency and the cyclical stability of battery, greatly have impact on this kind of material
Actual application.And prepared by structure regulating and there is the Tin monoxide of special construction (lamellar, porous etc.) one
Determine in degree, to alleviate Tin monoxide volumetric expansion in charge and discharge process.Further, Tin monoxide is Nonequilibrium Materials,
Can not directly obtain from nature.Therefore, a kind of method simply is used to prepare the Tin monoxide with special appearance
Have great importance.
According to reported in literature, the preparation method of Tin monoxide mainly includes spray burning method, hydrothermal synthesis method etc..Li Chunzhong
Et al. with stannous octoate as raw material, use spray burning method be prepared for the Tin monoxide of nano-sheet as lithium ion battery
Negative material, shows cyclical stability (Li Chunzhong, Hu Yanjie, Kong Lingyan etc., a kind of Tin monoxide of excellence
The preparation method of nanometer sheet, Chinese Patent Application No.: 201210153297.6).Compared with spray burning method, hydro-thermal is closed
One-tenth method has the advantages such as equipment is simple, mild condition is controlled.Sun Guang et al. is with cetyl trimethylammonium bromide as template
Agent, use hydro-thermal method prepared have honey comb structure Tin monoxide (Sun Guang, Li Yanwei, Cao Jianliang etc., one
Plant the preparation method of honeycomb Tin monoxide nano material, Chinese Patent Application No.: 201210157920.5), with ethanol
(Sun Guang, Li Yanwei, Cao Jianliang etc., one prepares porous spherical oxygen to have prepared porous spherical Tin monoxide for solvent
Change stannous nano material method, Chinese Patent Application No.: 201210157927.7).Visible, Hydrothermal Synthesis is that one obtains
Obtain the effective ways of Tin monoxide nano material.But at present about the report of water heat transfer Tin monoxide nano material
Relatively fewer, how by the regulation of hydrothermal process, preparation has the Tin monoxide nano material of special appearance and is still mesh
The study hotspot of front nanometer synthesis technical field.
Summary of the invention
It is an object of the invention to provide the preparation method of the Tin monoxide material of a kind of shelly texture.
For reaching above-mentioned purpose, present invention employs techniques below scheme:
1) by 1.128～4.512g SnCl2·2H2O adds in 50～90mL deionized waters and stirring and dissolving obtains solution A,
Adding reducing agent in solution A, then supersound process 10～30min obtains solution A 1, described SnCl2·2H2O and reduction
The mass ratio of agent is 0.31～3.76:1, uses NH3·H2Stir 5～10min after the pH to 7～8 of O regulation solution A 1 to obtain
To mixed liquor；
2) mixed liquor is transferred in politef water heating kettle, and in described water heating kettle, is full of nitrogen, then by institute
Stating water heating kettle to be placed in homogeneous reactor, then react 5～10h at 120～180 DEG C, reaction terminates rear natural cooling
To room temperature, then separated, by true for the precipitation of isolated by the centrifugal precipitation (grey black powder body) that reaction is obtained
Vacuum freecing-dry obtains Tin monoxide material.
Described reducing agent is citric acid, oxalic acid or hydrazine hydrate.
Sn in described solution A 12+Concentration be 0.05～0.4mol L-1。
The ultrasonic power that described supersound process uses is 40～100W.
Described NH3·H2The concentration of O is 14.8mol L-1。
The compactedness of described water heating kettle controls 50～90%.
The condition of described vacuum lyophilization is :-50 DEG C, 20Pa and 8～12h.
Described Tin monoxide material be particle diameter be the Tin monoxide powder body of the shelly texture of 10～20 μm, shelly texture
By the lamellar body composition that thickness is 1～2 μm.
Beneficial effects of the present invention is embodied in:
The present invention is using water as solvent, with SnCl2·2H2O is as Xi Yuan, and citric acid etc. is as reducing agent.Use a step
Hydro-thermal method is prepared for the Tin monoxide powder body of the shelly texture that particle diameter is 10～20 μm, and the oxidation of shelly texture is sub-
Stannum is by sheet that thickness is 1～2 μm composition, and purity is high, additionally, preparation method of the present invention is simple, reaction temperature is low,
Repeatability is high, the cycle is short, energy consumption is low, is suitable for large-scale production and application.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the Tin monoxide powder body of the shelly texture prepared by embodiment 3；
Fig. 2 is that scanning electron microscope (SEM) photo of the Tin monoxide powder body of the shelly texture prepared by embodiment 3 is (low
Figure again)；
Fig. 3 is that scanning electron microscope (SEM) photo of the Tin monoxide powder body of the shelly texture prepared by embodiment 3 is (high
Figure again).
Detailed description of the invention
With embodiment, the present invention is elaborated below in conjunction with the accompanying drawings.
Embodiment 1
1) by 1.128g SnCl2·2H2O adds 1.2g citric acid after being dissolved in 50mL deionized water, the most ultrasonic
Process 10min (80W) and obtain solution A 1, Sn in solution A 12+Concentration be 0.1mol L-1, then in solution A 1
Dropping concentration is 14.8mol L-1Dense NH3·H2The pH of O regulation solution is 7, stirs 5min the most at room temperature
Obtain uniform mixed liquor；
2) being transferred in politef water heating kettle by mixed liquor obtained above, compactedness is 50%, and at water heating kettle
In be full of nitrogen be placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A), at 120 DEG C
At a temperature of react 10h, reaction naturally cools to room temperature after terminating, and is then separated by grey black powder body by centrifugal, will
The vacuum powder lyophilization (-50 DEG C, 20Pa and 10h) of isolated obtains Tin monoxide powder body；
3) with Rigaku D/max2000PCX-x ray diffractometer x analyze sample (Tin monoxide powder body), find sample with
The SnO structure of the numbered 78-1913 of JCPDS is consistent, by this sample Flied emission of FEI Co. of U.S. S-4800 type
Scanning electron microscope (FESEM) is observed, it can be seen that prepared Tin monoxide powder body is that size is about 20
The shelly texture of μm, and the Tin monoxide of shelly texture is by the sheet composition that thickness is 1～2 μm.
Embodiment 2
1) by 2.256g SnCl2·2H2O adds 3.6g citric acid after being dissolved in 50mL deionized water, the most ultrasonic
Process 20min (100W) and obtain solution A 1, Sn in solution A 12+Concentration be 0.2mol L-1, then to solution A 1
Middle dropping concentration is 14.8mol L-1Dense NH3·H2The pH of O regulation solution is 8, stirs 10min the most at room temperature
Obtain uniform mixed liquor；
2) being transferred in politef water heating kettle by mixed liquor obtained above, compactedness is 50%, and at water heating kettle
In be full of nitrogen be placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A), at 160 DEG C
At a temperature of react 10h, reaction naturally cools to room temperature after terminating, and is then separated by grey black powder body by centrifugal, will
The vacuum powder lyophilization (-50 DEG C, 20Pa and 12h) of isolated obtains Tin monoxide powder body；
3) with Rigaku D/max2000PCX-x ray diffractometer x analyze sample (Tin monoxide powder body), find sample with
The SnO structure of the numbered 78-1913 of JCPDS is consistent, by this sample Flied emission of FEI Co. of U.S. S-4800 type
Scanning electron microscope (FESEM) is observed, it can be seen that prepared Tin monoxide powder body is that size is about 20
The shelly texture of μm, and the Tin monoxide of shelly texture is by the sheet composition that thickness is 1～2 μm.
Embodiment 3
1) by 1.128g SnCl2·2H2O is dissolved in 50mL deionized water addition 2.4g citric acid the most afterwards, the most ultrasonic
Process 10min (50W) and obtain solution A 1, Sn in solution A 12+Concentration be 0.1mol L-1, then in solution A 1
Dropping concentration is 14.8mol L-1Dense NH3·H2The pH of O regulation solution is 7.5, stirs 5min the most at room temperature
Obtain uniform mixed liquor；
2) being transferred in politef water heating kettle by mixed liquor obtained above, compactedness is 50%, and at water heating kettle
In be full of nitrogen be placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A), at 180 DEG C
At a temperature of react 5h, reaction naturally cools to room temperature after terminating, and is then separated by grey black powder body by centrifugal, will point
Tin monoxide powder body is obtained from the vacuum powder lyophilization (-50 DEG C, 20Pa and 10h) obtained；
3) with Rigaku D/max2000PCX-x ray diffractometer x analyze sample (Tin monoxide powder body), find sample with
The SnO structure of the numbered 78-1913 of JCPDS is consistent, sees Fig. 1；By this sample FEI Co. of U.S. S-4800
The field emission scanning electron microscope (FESEM) of type is observed, it can be seen that prepared Tin monoxide powder body is
Size is about the shelly texture of 20 μm, and the Tin monoxide of shelly texture is by the sheet composition that thickness is 1～2 μm,
See Fig. 2 and Fig. 3.
Embodiment 4
1) by 4.512g SnCl2·2H2O adds 2.4g citric acid after being dissolved in 80mL deionized water, the most ultrasonic
Process 30min (100W) and obtain solution A 1, Sn in solution A 12+Concentration be 0.25mol L-1, then to solution A 1
Middle dropping concentration is 14.8mol L-1Dense NH3·H2The pH of O regulation solution is 7.5, stirs 10 the most at room temperature
Min obtains uniform mixed liquor；
2) being transferred in politef water heating kettle by mixed liquor obtained above, compactedness is 80%, and at water heating kettle
In be full of nitrogen be placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A), at 180 DEG C
At a temperature of react 8h, reaction naturally cools to room temperature after terminating, and is then separated by grey black powder body by centrifugal, will point
Tin monoxide powder body is obtained from the vacuum powder lyophilization (-50 DEG C, 20Pa and 12h) obtained；
3) with Rigaku D/max2000PCX-x ray diffractometer x analyze sample (Tin monoxide powder body), find sample with
The SnO structure of the numbered 78-1913 of JCPDS is consistent, by this sample Flied emission of FEI Co. of U.S. S-4800 type
Scanning electron microscope (FESEM) is observed, it can be seen that prepared Tin monoxide powder body is that size is about 20
The shelly texture of μm, and the Tin monoxide of shelly texture is by the sheet composition that thickness is 1～2 μm.
Embodiment 5
1) by 2.256g SnCl2·2H2O adds 1.2g citric acid, the most ultrasonic place after being dissolved in 60mL deionized water
Reason 10min (60W) obtains solution A 1, Sn in solution A 12+Concentration be 0.17mol L-1, then in solution A 1
Dropping concentration is 14.8mol L-1Dense NH3·H2The pH of O regulation solution is 8, stirs 8min the most at room temperature
Obtain uniform mixed liquor；
2) being transferred in politef water heating kettle by mixed liquor obtained above, compactedness is 60%, and at water heating kettle
In be full of nitrogen be placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A), at 140 DEG C
At a temperature of react 6h, reaction naturally cools to room temperature after terminating, and is then separated by grey black powder body by centrifugal, will point
Tin monoxide powder body is obtained from the vacuum powder lyophilization (-50 DEG C, 20Pa and 10h) obtained；
3) with Rigaku D/max2000PCX-x ray diffractometer x analyze sample (Tin monoxide powder body), find sample with
The SnO structure of the numbered 78-1913 of JCPDS is consistent, by this sample Flied emission of FEI Co. of U.S. S-4800 type
Scanning electron microscope (FESEM) is observed, it can be seen that prepared Tin monoxide powder body is that size is about 20
The shelly texture of μm, and the Tin monoxide of shelly texture is by the sheet composition that thickness is 1～2 μm.
The present invention is using water as solvent, with SnCl2·2H2O is as Xi Yuan, and citric acid etc. is as reducing agent.Use a step
Hydro-thermal method is prepared for the Tin monoxide powder body that particle diameter is about the shelly texture of 20 μm, and this shelly texture is multilayer tablet
The assembling of shape structure, owing to its structure is special, can be applicable to lithium/anode material of lithium-ion battery, chemosynthesis catalyst
Etc. aspect.It addition, preparation method of the present invention is simple, reaction temperature height low, repeated, the cycle is short, energy consumption is low, suitable
Close large-scale production and application.
Claims (7)
1. the preparation method of the Tin monoxide material of a shelly texture, it is characterised in that: comprise the following steps:
1) by 1.128～4.512g SnCl2·2H2O adds in 50～90mL deionized waters and stirring and dissolving obtains solution A,
Adding reducing agent in solution A, then supersound process 10～30min obtains solution A 1, described SnCl2·2H2O and reduction
The mass ratio of agent is 0.31～3.76:1, uses NH3·H2Stir 5～10min after the pH to 7～8 of O regulation solution A 1 to obtain
To mixed liquor；
2) mixed liquor is transferred in politef water heating kettle, and in described water heating kettle, is full of nitrogen, then by institute
Stating water heating kettle to be placed in homogeneous reactor, then react 5～10h at 120～180 DEG C, reaction terminates rear natural cooling
To room temperature, then by the centrifugal precipitate and separate that reaction is obtained, the precipitation vacuum lyophilization of isolated is obtained
Tin monoxide material；
Described reducing agent is citric acid, oxalic acid or hydrazine hydrate.
A kind of preparation method of the Tin monoxide material of shelly texture, it is characterised in that:
Sn in described solution A 12+Concentration be 0.05～0.4mol L-1。
A kind of preparation method of the Tin monoxide material of shelly texture, it is characterised in that:
The ultrasonic power that described supersound process uses is 40～100W.
A kind of preparation method of the Tin monoxide material of shelly texture, it is characterised in that:
Described NH3·H2The concentration of O is 14.8mol L-1。
A kind of preparation method of the Tin monoxide material of shelly texture, it is characterised in that:
The compactedness of described water heating kettle controls 50～90%.
A kind of preparation method of the Tin monoxide material of shelly texture, it is characterised in that:
The condition of described vacuum lyophilization is :-50 DEG C, 20Pa and 8～12h.
A kind of preparation method of the Tin monoxide material of shelly texture, it is characterised in that:
Described Tin monoxide material be particle diameter be the Tin monoxide powder body of the shelly texture of 10～20 μm, shelly texture is equal
It is made up of the lamellar body that thickness is 1～2 μm.
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| CN105819499B (en) * | 2016-03-23 | 2017-05-10 | 昆明理工大学 | Preparation method of stannous oxide particles with photocatalytic activity |
| CN106966426B (en) * | 2017-04-21 | 2018-11-16 | 浙江百传网络科技有限公司 | A kind of preparation method of nanoporous stannous oxide |
| CN107819148B (en) * | 2017-10-31 | 2019-06-25 | 杭州电子科技大学 | A kind of SnO with partial size bimodal distribution2Nanosphere and its application |
| CN112607765A (en) * | 2021-01-25 | 2021-04-06 | 严永生 | Method for preparing stannous fluoride by adopting freeze drying |
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| CN102659177B (en) * | 2012-05-21 | 2014-04-09 | 河南理工大学 | Method for preparing porous spherical stannous oxide nano material |
| CN102659176B (en) * | 2012-05-21 | 2014-03-05 | 河南理工大学 | Method for preparing comby stannous oxide nanometer material |
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